CN107512708A - A kind of recovery method of ultra-high purity nitrous oxide - Google Patents
A kind of recovery method of ultra-high purity nitrous oxide Download PDFInfo
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- CN107512708A CN107512708A CN201610436372.8A CN201610436372A CN107512708A CN 107512708 A CN107512708 A CN 107512708A CN 201610436372 A CN201610436372 A CN 201610436372A CN 107512708 A CN107512708 A CN 107512708A
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- tail gas
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/22—Nitrous oxide (N2O)
Abstract
The invention discloses a kind of recovery method of ultra-high purity nitrous oxide, this comprises the following steps：Step S1, the tail gas containing nitrous oxide is subjected to three-level carrying out washing treatment by one-stage water wash device and two-stage organic solvent washing device successively；Step S2, tail gas is subjected to cooling treatment through heat exchanger；Step S3, tail gas is subjected to two-stage adsorption treatment through pressure-swing absorption apparatus and temperature swing absorption unit successively；Step S4, tail gas is subjected to two stage rectification processing through one-level rectifying column and two-stage rectification tower successively.Due to the organic coordinated of each step of the present invention, therefore nitrous oxide in tail gas can be completely separated, so as to obtain the ultra-high purity nitrous oxide gas that purity is not less than 99.99999%, not only meet in industry and laboratory the needs of for more than purity alumina Asia nitrogen, and drastically reduce the area because of the discharge of nitrous oxide and pollution on the environment；The method of the present invention recycles nitrous oxide, is wasted so as to avoid, has saved resource.
Description
Technical field
The present invention relates to a kind of recovery method of nitrous oxide, more particularly to a kind of recovery method of ultra-high purity nitrous oxide.
Background technology
Nitrous oxide is also known as laughing gas, is a kind of colourless pleasantly sweet gaseous oxidant because its can resolve at high temperature nitrogen and
Oxygen, therefore can support to burn under certain condition.But its stable performance at room temperature, there is light anaesthesia effect, and energy
Cause people to laugh, be primarily now used to perform.Part of in August, 2009, one, U.S. current research show that nitrous oxide has become
The primary ODS of mankind's discharge, its unimolecule heat 310 times that potentiality is carbon dioxide, it has also become《Discuss in capital of a country
Agreement》Specified in 6 kinds cause one of gas of greenhouse effects.
Nitrous oxide mostlys come from production and the life process of the mankind.Wherein most important source is the tail gas in chemical industry,
Such as nylon, nitric acid production process, due to containing substantial amounts of nitrous oxide in the tail gas discharged from these process units, therefore
If can not properly be processed to, serious environmental problem will certainly be brought.
Currently used processing method be by these above-mentioned tail gas with being discharged after charcoal absorption, because processing means are relatively simple and
Not thoroughly, therefore in the tail gas after processing substantial amounts of nitrous oxide is still contained, so can not solve the problems, such as welding, and not
Nitrous oxide can be recycled, so as to cause to waste.In addition, although in the prior art it has been reported that being related to oxidation Asia
Some other method of nitrogen purifying, but the purity of resulting nitrous oxide is not higher than 99.9999%, it is difficult to meet current work
The actual demand of ultra-high purity nitrous oxide of the purity not less than 99.99999% is needed to use in industry and laboratory.
For this reason, the present inventor is studied, it is therefore an objective to is solved association area prior art and is exposed
The problem of, it is expected to provide a kind of recovery method of ultra-high purity nitrous oxide, to obtain the oxidation that purity is not less than 99.99999%
Sub- nitrogen.
The content of the invention
In view of above the deficiencies in the prior art, it is an object of the invention to provide a kind of recovery method of ultra-high purity nitrous oxide.
Present inventor by after many experiments and creative work it was unexpectedly observed that in three-level carrying out washing treatment, cooling treatment, two
Level adsorption treatment and two stage rectification are handled under the synergy of these steps, and method of the invention can obtain purity and be not less than
99.99999% ultra high purity nitric oxide Asia nitrogen.
The invention provides a kind of method for reclaiming and purifying nitrous oxide in industrial tail gas, it includes：
Step S1, the tail gas containing nitrous oxide is carried out three by one-stage water wash device and two-stage organic solvent washing device successively
Level carrying out washing treatment；
Step S2, tail gas is subjected to cooling treatment through heat exchanger；
Step S3, tail gas is subjected to two-stage adsorption treatment through pressure-swing absorption apparatus and temperature swing absorption unit successively；
Step S4, tail gas is subjected to two stage rectification processing through one-level rectifying column and two-stage rectification tower successively.
According to the specific embodiment of the present invention, the N described in step S1 in tail gas2O content is 0.1~4% (v/v),
It is preferred that 1~4% (v/v).
According to the specific embodiment of the present invention, the one-stage water wash device includes water scrubber and is connected with the water scrubber
Regeneration water storage tank；After tail gas flows into water scrubber, it is eluted using washings, washings are flowed into from washing tower bottom
Regenerate in water storage tank, flow back into water scrubber and recycled again after evacuated parsing；Wherein, the regeneration water storage tank
Vacuum is not higher than -0.05MPa, preferably -0.06~-0.08MPa.
According to the specific embodiment of the present invention, the organic solvent used in the two-stage organic solvent washing device is respectively selected from
Polyethylene glycol dimethyl ether, propene carbonate and methanol, are preferably selected from NHD and propene carbonate.
According to the specific embodiment of the present invention, the tail gas is after one-stage water wash washs the carrying out washing treatment of device, wherein CO2Contain
Amount is reduced within 1% (v/v)；The tail gas is again after two-stage organic solvent washing device carrying out washing treatment, wherein CO2Content
It is reduced within 3ppm (v/v).
According to the specific embodiment of the present invention, tail gas is cooled to 3~5 DEG C of temperature after heat exchanger exchanges heat in step S2,
It is preferred that 3.5 DEG C~4.5 DEG C, more preferably 3.8 DEG C.
According to the specific embodiment of the present invention, first by after the pressure boost of tail gas to 1.0MPa~1.1MPa in step S3
Two-stage adsorption treatment is carried out again.
According to the specific embodiment of the present invention, it is characterised by, pressure-swing absorption apparatus described in step S3 is transformation dryer,
The drier wherein used is 4A molecular sieves；Tail gas is after pressure-swing absorption apparatus adsorption treatment, wherein H2O content is reduced to 3ppm
(v/v) within.
According to the specific embodiment of the present invention, temperature swing absorption unit is temperature-change adsorption tower described in step S3, wherein use
Adsorbent is the modified molecular screen that aperture is less than 0.1nm；Tail gas is after temperature swing absorption unit adsorption treatment, wherein CO2Content is small
In 0.1ppm (v/v), C2H2Content is less than 0.05ppm (v/v).
According to the specific embodiment of the present invention, one-level rectifying column described in step S4 is packed tower, and the number of plates is more than 6 pieces,
Feed tray number is more than 5 pieces, and reflux ratio is more than 0.2.
According to the specific embodiment of the present invention, the temperature of the overhead condenser of one-level rectifying column is not higher than described in step S4
- 60 DEG C, preferably -65 DEG C；The temperature of tower bottom reboiler is not less than -35 DEG C, preferably -25 DEG C.
According to the specific embodiment of the present invention, the gas inlet flow of one-level rectifying column is described in step S4
800~1600Nm3/ h, preferably 1000~1400Nm3/ h, more preferably 1100~1200Nm3/h；Overhead gas discharge capacity is
800~1300Nm3/ h, preferably 900~1200Nm3/ h, more preferably 1000~1100Nm3/h；Tower reactor gas emissions are
0.02~0.1Nm3/ h, preferably 0.04~0.08Nm3/ h, more preferably 0.05~0.07Nm3/h。
According to the specific embodiment of the present invention, two-stage rectification tower described in step S4 is packed tower, and the number of plates is more than 8 pieces,
Feed tray number is more than 3 pieces, and reflux ratio is more than 0.6.
According to the specific embodiment of the present invention, the temperature of the overhead condenser of two-stage rectification tower is not higher than described in step S4
- 95 DEG C, preferably -98 DEG C；The temperature of tower bottom reboiler is not less than -45 DEG C, preferably -40 DEG C.
According to the specific embodiment of the present invention, the gas inlet flow of two-stage rectification tower is described in step S4
650~1400Nm3/ h, preferably 800~1200Nm3/ h, more preferably 1000~1100Nm3/h；Overhead gas discharge capacity is
400~950Nm3/ h, preferably 600~800Nm3/ h, more preferably 650~750Nm3/h；Tower reactor gas emissions are 0.3~0.8Nm3/ h,
It is preferred that 0.4~0.6Nm3/ h, more preferably 0.45~0.55Nm3/h。
According to the specific embodiment of the present invention, tail gas described in step S1 includes N2、O2、Ar、H2O、NO、N2O、
NO2、NH3、CO、CO2、C1~C6Organic matter, C6 benzene derivatives and combinations thereof；Wherein, N2O content is 10~50%
(v/v), preferably 30~40% (v/v).
According to the specific embodiment of the present invention, impurity described in step S1 contains C6 benzene derivatives, the C6 benzenesulfonamide derivatives
Thing includes but is not limited to aniline, nitrobenzene and benzoic acid.
According to the specific embodiment of the present invention, the purity of the nitrous oxide obtained by the method for the invention recovery tail gas is not low
In 99.99999%.
In the method for the invention, the purity of nitrous oxide gas detects to obtain by following instruments：Pulsed Discharge Helium ion
Change detector (PDHID), flame ionization detector (FID), cavity ring down spectroscopy technology (CRDS), Moisture Meter, red
External spectrum instrument and gas chromatograph.
The production method of nitrous oxide mainly has ammonium nitrate thermal decomposition method, ammonia catalytic method and urea method etc..Especially, exist
, can be by containing nitrous oxide to caused during production nitric acid or adipic acid in the manufacturing enterprise of nitric acid and adipic acid
Tail gas is handled to reclaim nitrous oxide.
According to the specific embodiment of the present invention, the tail gas containing nitrous oxide and impurity described in step S1 can come industrial
Caused waste gas or produced in adipic acid production process during preparing cyclohexanone oxime with ammonia and hydroperoxidation by cyclohexanone
Raw waste gas.
Beneficial effects of the present invention：Due to the organic coordinated of each step of the present invention, therefore oxygen in tail gas can be completely separated
Change sub- nitrogen, so as to obtain the ultra-high purity nitrous oxide gas that purity is not less than 99.99999%, not only meet industry and laboratory
In for the demand more than purity alumina Asia nitrogen, and drastically reduce the area because of the discharge of nitrous oxide and pollution on the environment；
The method of the present invention recycles nitrous oxide, is wasted so as to avoid, has saved resource；In addition, the method for the present invention
Automaticity is high, and can continuous production, so treating capacity is big, therefore have broad application prospects.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, in being described below to embodiment it is required use it is attached
Figure, which is done, simply to be introduced, it is therefore apparent that the accompanying drawing in brief description is only some embodiments of the present invention, general for this area
For logical technical staff, on the premise of not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 represents to realize the schematic diagram of a preferred embodiment of the inventive method.In figure, identical component is by identical accompanying drawing
Mark sign.Accompanying drawing is not drawn according to the ratio of reality.Reference is described as follows：
1 one-stage water wash tower；
2 first order organic solvent washing towers；
3 second level organic solvent washing towers；
4 heat exchangers；
5 surge tanks；
6 compression pumps；
7 pressure-swing absorption apparatus；
8 temperature swing absorption units；
9 first order rectifying columns；
10 second level rectifying columns；
11 regeneration water storage tanks；
12 first organic solvents regenerate storage tank；
13 second organic solvents regenerate storage tank；
Embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, it will be appreciated by those skilled in the art that
The following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted actual conditions person in embodiment,
The condition suggested according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, are to pass through
The conventional products of acquisition purchased in market.
As shown in figure 1, the present apparatus includes one-stage water wash tower 1, first order organic solvent washing tower 2, second level organic solvent successively
Scrubbing tower 3, heat exchanger 4, surge tank 5, compression pump 6, pressure-swing absorption apparatus 7, temperature swing absorption unit 8, first order rectifying column
9 and second level rectifying column 10.
The tail gas used in the present embodiment, the testing result of wherein each component content are as shown in table 1 below：
Table 1
| Exhaust gas composition | Constituent content (V/V) | Content analysis method | Equipment manufacturer |
| N2O | 30.24% | PDHID | Valco |
| O2+Ar | 6.4% | PDHID | Valco |
| N2 | 47.60% | PDHID | Valco |
| CO | 0.16% | PDHID | Valco |
| CO2 | 7.2% | PDHID | Valco |
| H2O | 2.4% | CRDS | HALO |
| NOX | 90ppm | FID | Valco |
| C1~C6 organic matters | 20ppm | PDHID | Valco |
After tail gas containing each component content in upper table 1 is flowed into water scrubber 1, tail gas is eluted first with washings,
Washings are flowed into vacuum degree control in -0.07MPa regeneration water storage tank 11 from the bottom of water scrubber 1；Evacuated parsing
Afterwards, washings are back in water scrubber 1 again carries out cycling and reutilization.CO in tail gas after elution2Content is reduced to 1% (v/v)
Within, tail gas is flowed into first order organic solvent washing tower 2 from the tower top of water scrubber.
Detergent of the NHD as tail gas is used in first order organic solvent washing tower 2, for getting rid of in tail gas
The CO of residual2Impurity.First order organic solvent washing tower 2 is connected with the first organic solvent regeneration storage tank 12.For washing tail gas
Polyethylene glycol dimethyl ether from the bottom of first order organic solvent washing tower 2 be flowed into organic solvent regeneration storage tank 12 in, it is evacuated
Recycled again from overhead reflux into first order organic solvent washing tower 2 after parsing.
Tail gas is after first order organic solvent washing, wherein CO2Content be further decreased within 10ppm (v/v), its
Flowed into from the tower top of first order organic solvent washing tower 2 in second level organic solvent washing tower 3.
Detergent of the NHD as tail gas is used in second level organic solvent washing tower 3, for further getting rid of
The CO of trace in tail gas2Impurity.Second level organic solvent washing tower 3 is also connected with an organic solvent regeneration storage tank 13.For
NHD after washing tail gas is flowed into solvent reclamation storage tank 13 from the bottom of second level organic solvent washing tower 3,
Recycled again from overhead reflux into second level organic solvent washing tower 3 after evacuated parsing.
Tail gas is after the organic solvent washing of the second level, wherein CO2Content is further reduced within 1ppm (v/v), and it is from
The tower top of two level organic solvent washing tower 3 is flowed into heat exchanger 4.
Tail gas after three-level is washed is introduced into heat exchanger 4 and carries out heat exchange cooling, and gas temperature is reduced to 3.8 DEG C, for by tail gas
The NHD organic solvent of middle entrainment is effectively reclaimed.Organic solvent after recovery flows into from the bottom of heat exchanger 4
In one organic solvent recovery storage tank.Wherein, the cooling problem of gas needs strict control, effectively could so remove in tail gas
The NHD organic solvent of entrainment.
The tail gas flowed out from heat exchanger 4 enters back into and pressurized treatment is carried out in compressor 6 after the buffering of surge tank 5, pressure
Power increases to 0.55MPa, is then fed into transformation dryer 7 and carries out pressure-variable adsorption processing, and the water in tail gas is removed for depth.
The transformation dryer 7 is to reach drying effect by " pressure change ".Because tail gas accommodates the ability and pressure of steam
Power is inversely proportional, and its dried a part of tail gas (being referred to as regeneration gas) puffing to atmospheric pressure, this pressure change makes expansion
Tail gas becomes drier, then allows it to flow through the desiccant layer of the need of access failure air-flow regeneration and (has absorbed the drying of enough steam
Tower), dry regeneration gas suctions out the moisture content in drier, takes it out drier to reach the purpose of dehumidification.Two absorbing cylinders follow
Ring works, without thermal source, so as to fully dry the steam in tail gas.In the present embodiment, drier uses Al2O3Point
Son sieve, the volume of two absorbing cylinders are more than 1m3, pressure swing regeneration switching time was more than 5 minutes.Tail gas is through transformation dryer 7
After adsorption treatment, wherein H2O content is reduced within 3ppm (v/v).
Tail gas flows into progress temp.-changing adsorption processing in temperature-change adsorption tower 8 again after pressure-variable adsorption removes water process, and tail is removed for depth
CO in gas2And C2H2Impurity.The adsorbent used in temperature-change adsorption tower 8 is that footpath is less than 0.1 nano modification molecular sieve, and is contained
There are the rare metals such as metallic nickel, palladium, platinum.The modified molecular screen only optionally CO in absorption tail gas2And C2H2Impurity,
Without N in absorption tail gas20.Tail gas is after the adsorption treatment of temperature-change adsorption tower 8, wherein CO2Content is less than 0.1ppm (v/v),
C2H2Content is less than 0.05ppm (v/v).
The tail gas flowed out from heat exchanger 4 flows into first order rectifying column 9 after the cushioning effect of a surge tank and carries out one-level
Rectification process.In the present embodiment, first order rectifying column 9 is packed tower.In the present invention, the number of plates of packed tower and backflow
The recovery purity for comparing nitrous oxide has particularly important influence, it is necessary to carries out strict control.Present inventor passes through
Found after many experiments and creative work, the number of plates of first order rectifying column is more than 6 pieces, and feed tray number is more than 5 pieces, returns
Stream is than being more than 0.2.Specifically, in the present embodiment, the number of plates of first order rectifying column is 8 pieces, and feed tray number is 6 pieces,
Reflux ratio is 0.3.
In the present embodiment, the overhead condenser temperature of first order rectifying column is -65 DEG C；Tower bottom reboiler temperature is -25 DEG C.Tail gas
≤ -50 DEG C are cooled in the condenser of tower top, now, including H2O、NO2、C3H8、C3H6、C4H10、C5H12、
NH3、C6Impurity (i.e. high-boiling-point impurity) of the boiling point higher than -50 DEG C including benzene derivative and organic solvent is then condensed into liquid；
And including H2、N2、O2、CO、Ar、NO、CH4、C2H4And N2Boiling point including O is (i.e. low less than -50 DEG C of impurity
Boiling contaminants) then remain as gas.Liquid is enriched with tower reactor reboiler, and this part of main component is very small amount N2O and upper
High boiling impurity is stated, it discharges first order rectifying column 9 as waste gas from reboiler sewage draining exit.Meanwhile the low boiling impurity
(H2、N2、O2、CO、Ar、NO、CH4、C2H4And N2O) and the overwhelming majority N2O remains as gas, its from
The tower top outlet of first order rectifying column 9 is discharged enters second level rectifying column 10 by pipeline.
In the present embodiment, second level rectifying column 10 is also packed tower, and the number of plates and reflux ratio of packed tower are returned to nitrous oxide
Receiving purity has important influence.Present inventor after many experiments and creative work by having found, second level rectifying column
The number of plates be more than 8 pieces, feed tray number be more than 3 pieces, reflux ratio be more than 0.6.Specifically, in the present embodiment, the second level
The number of plates of rectifying column is 10 pieces, and feed tray number is 5 pieces, reflux ratio 0.8.
In the present embodiment, the overhead condenser temperature of second level rectifying column 10 is -98 DEG C；Tower bottom reboiler temperature is -40 DEG C.
Now, boiling point is higher than -88.5 DEG C of N2O is condensed into liquid, and boiling point is less than -88.5 DEG C of impurity, including H2、N2、O2、
CO、Ar、C2H4、NO、CH4Gas is remained as, they are enriched with tower top, and discharge rectifying from tower top outlet as waste gas
Tower, this portion also include the N that very small amount is not liquefied2O；And the N being liquefied in tail gas20 flows into tower reactor again
Device is boiled, it discharges second level rectifying column 10 as final products.
In the present embodiment, the control of first order rectifying column 9 and 10 respective gas flow of second level rectifying column is very important side
Face is, it is necessary to carry out strict control.Table 2 below show first order rectifying column 9 and gas in second level rectifying column 10 in the present embodiment
Body flow control parameter.
Table 2
| Gas inlet flow/Nm3/h | Other discharge capacity/Nm of tower top3/h | Other discharge capacity/Nm of tower reactor3/h | |
| First order rectifying column 9 | 1150 | 1050 | 0.06 |
| Second level rectifying column 10 | 950 | 1060 | 0.5 |
The N that the method for this implementation is prepared2The detection and analysis result of O gas purities is as shown in table 3 below：
Table 3
| Composition | Analysis result | Analysis method | Analytical equipment |
| N2O | 99.99999% | PDHID | Valco |
| O2+Ar | ≤0.1ppmv | PDHID | Valco |
| N2 | ≤0.2ppmv | PDHID | Valco |
| CO | ≤0.05ppmv | PDHID | Valco |
| CO2 | ≤0.1ppmv | PDHID | Valco |
| H20 | ≤0.2ppmv | CRDS | HALO |
| C1~C6 organic matters | ≤0.1ppmv | FID | Valco |
| NO | ≤0.1ppmv | PDHID | Valco |
| NO2 | ≤0.1ppmv | FTIR | NICOLET IGS |
| NH3 | ≤0.1ppmv | PDHID | Valco |
It should be noted that embodiment described above is only used for explaining the present invention, any limitation of the invention is not formed.
By referring to exemplary embodiments, invention has been described, it should be appreciated that word wherein used is descriptive and explanatory
Vocabulary, rather than limited vocabulary.The present invention can be modified within the scope of the claims by regulation, and
The present invention is revised in without departing substantially from scope and spirit of the present invention.Although the present invention described in it be related to specific method,
Material and embodiment, it is not intended that the present invention is limited to wherein disclosed particular case, on the contrary, the present invention can be extended to other
All methods and applications with identical function.
Claims (16)
1. a kind of recovery method of ultra-high purity nitrous oxide, it includes：
Step S1, the tail gas containing nitrous oxide is carried out three by one-stage water wash device and two-stage organic solvent washing device successively
Level carrying out washing treatment；
Step S2, tail gas is subjected to cooling treatment through heat exchanger；
Step S3, tail gas is subjected to two-stage adsorption treatment through pressure-swing absorption apparatus and temperature swing absorption unit successively；
Step S4, tail gas is subjected to two stage rectification processing through one-level rectifying column and two-stage rectification tower successively.
2. according to the method described in claim 1, it is characterised in that the one-stage water wash device include water scrubber and with institute
State the regeneration water storage tank that water scrubber is connected；After tail gas flows into water scrubber, it is eluted using washings, washings are from water
Wash tower bottom to be flowed into regeneration water storage tank, flow back into water scrubber and recycled again after evacuated parsing；Wherein, institute
The vacuum for stating regeneration water storage tank is not higher than -0.05MPa, preferably -0.06~-0.08MPa.
3. the method according to any one in claim 1~2, it is characterised in that the two-stage organic solvent washing device
The middle organic solvent used is respectively selected from NHD, propene carbonate and methanol, be preferably selected from polyethylene glycol dimethyl ether and
Propene carbonate.
4. the method according to any one in claims 1 to 3, it is characterised in that the tail gas washs device through one-stage water wash
Carrying out washing treatment after, wherein CO2Content is reduced within 1% (v/v)；The tail gas is again through two-stage organic solvent washing device
After carrying out washing treatment, wherein CO2Content is reduced within 1ppm (v/v).
5. the method according to any one in Claims 1 to 4, it is characterised in that by tail gas through heat exchanger in step S2
3~5 DEG C of temperature, more preferably preferably 3.5 DEG C~4.5 DEG C, 3.8 DEG C are cooled to after heat exchange.
6. the method according to any one in Claims 1 to 5, it is characterised in that first by the pressure of tail gas in step S3
Power is pressurized to after 1.0MPa~1.1MPa carries out two-stage adsorption treatment again.
7. the method according to any one in claim 1~6, it is characterised in that pressure-variable adsorption described in step S3 fills
It is transformation dryer to put, wherein the drier used is 4A molecular sieves；Tail gas after pressure-swing absorption apparatus adsorption treatment, wherein
H2O content is reduced within 3ppm (v/v).
8. the method according to any one in claim 1~7, it is characterised in that temp.-changing adsorption described in step S3 fills
It is temperature-change adsorption tower to put, wherein the adsorbent used is the modified molecular screen that aperture is less than 0.1nm；Tail gas is through temperature swing absorption unit
After adsorption treatment, wherein CO2Content is less than 0.1ppm (v/v), C2H2Content is less than 0.05ppm (v/v).
9. the method according to any one in claim 1~8, it is characterised in that one-level rectifying column described in step S4
For packed tower, the number of plates is more than 6 pieces, and feed tray number is more than 5 pieces, and reflux ratio is more than 0.2.
10. the method according to any one in claim 1~9, it is characterised in that one-level rectifying column described in step S4
Overhead condenser temperature be not higher than -60 DEG C, preferably -65 DEG C；The temperature of tower bottom reboiler is not less than -35 DEG C, preferably -25 DEG C.
11. the method according to any one in claim 1~10, it is characterised in that one-level rectifying column described in step S4
Gas inlet flow be 800~1600Nm3/ h, preferably 1000~1400Nm3/ h, more preferably 1100~1200Nm3/h；Tower top
Gas emissions are 800~1300Nm3/ h, preferably 900~1200Nm3/ h, more preferably 1000~1100Nm3/h；Tower reactor gas
Discharge capacity is 0.02~0.1Nm3/ h, preferably 0.04~0.08Nm3/ h, more preferably 0.05~0.07Nm3/h。
12. the method according to any one in claim 1~11, it is characterised in that two-stage rectification tower described in step S4
For packed tower, the number of plates is more than 8 pieces, and feed tray number is more than 3 pieces, and reflux ratio is more than 0.6.
13. the method according to any one in claim 1~12, it is characterised in that two-stage rectification tower described in step S4
Overhead condenser temperature be not higher than -95 DEG C, preferably -98 DEG C；The temperature of tower bottom reboiler is not less than -45 DEG C, preferably -40 DEG C.
14. the method according to any one in claim 1~13, it is characterised in that two-stage rectification tower described in step S4
Gas inlet flow be 650~1400Nm3/ h, preferably 800~1200Nm3/ h, more preferably 1000~1100Nm3/h；Tower top
Gas emissions are 400~950Nm3/ h, preferably 600~800Nm3/ h, more preferably 650~750Nm3/h；Tower reactor gas discharges
Measure as 0.3~0.8Nm3/ h, preferably 0.4~0.6Nm3/ h, more preferably 0.45~0.55Nm3/h。
15. the method according to any one in claim 1~14, it is characterised in that tail gas includes described in step S1
N2、O2、Ar、H2O、NO、N2O、NO2、NH3、CO、CO2、C1~C6Organic matter, C6 benzene derivatives and its group
Close；Wherein, N2O content is 10~50% (v/v), preferably 30~40% (v/v).
16. the method according to any one in claim 1~15, it is characterised in that methods described reclaims obtained oxidation
The purity of sub- nitrogen is not less than 99.99999%.
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| CN (1) | CN107512708A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483415A (en) * | 2018-06-14 | 2018-09-04 | 北京万机汇机电工程技术有限公司 | A kind of device and method preparing nitrous oxide |
| CN110835101A (en) * | 2019-10-24 | 2020-02-25 | 河南神马尼龙化工有限责任公司 | Device and method for recovering electronic-grade nitrous oxide from industrial tail gas |
| CN111039266A (en) * | 2019-12-29 | 2020-04-21 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for removing nitrous oxide in nitrogen trifluoride |
| CN111302317A (en) * | 2020-04-02 | 2020-06-19 | 全椒科利德电子材料有限公司 | Continuous high-purity nitrous oxide production system and method |
| CN115524415A (en) * | 2022-09-16 | 2022-12-27 | 重庆同辉科发气体有限公司 | High-purity nitrous oxide analysis pipeline system |
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| CN105384154A (en) * | 2015-12-22 | 2016-03-09 | 苏州金宏气体股份有限公司 | Method for recycling and purifying nitrous oxide |
| CN105502317A (en) * | 2015-12-22 | 2016-04-20 | 苏州金宏气体股份有限公司 | Device for recycling and purifying nitrous oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105384154A (en) * | 2015-12-22 | 2016-03-09 | 苏州金宏气体股份有限公司 | Method for recycling and purifying nitrous oxide |
| CN105502317A (en) * | 2015-12-22 | 2016-04-20 | 苏州金宏气体股份有限公司 | Device for recycling and purifying nitrous oxide |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483415A (en) * | 2018-06-14 | 2018-09-04 | 北京万机汇机电工程技术有限公司 | A kind of device and method preparing nitrous oxide |
| CN110835101A (en) * | 2019-10-24 | 2020-02-25 | 河南神马尼龙化工有限责任公司 | Device and method for recovering electronic-grade nitrous oxide from industrial tail gas |
| CN110835101B (en) * | 2019-10-24 | 2023-01-31 | 河南神马尼龙化工有限责任公司 | Device and method for recovering electronic-grade nitrous oxide from industrial tail gas |
| CN111039266A (en) * | 2019-12-29 | 2020-04-21 | 中船重工（邯郸）派瑞特种气体有限公司 | Device and method for removing nitrous oxide in nitrogen trifluoride |
| CN111302317A (en) * | 2020-04-02 | 2020-06-19 | 全椒科利德电子材料有限公司 | Continuous high-purity nitrous oxide production system and method |
| CN115524415A (en) * | 2022-09-16 | 2022-12-27 | 重庆同辉科发气体有限公司 | High-purity nitrous oxide analysis pipeline system |
| CN115524415B (en) * | 2022-09-16 | 2023-05-30 | 重庆同辉科发气体有限公司 | High-purity nitrous oxide analysis pipeline system |
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